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Preparation method of highly sulfonated polystyrene resin

A technology of polystyrene resin and sulfonated polystyrene, which is applied in the field of functional modification of polymers, can solve the problems of low content of sulfonic acid groups on the surface, high cost, and low strength of resin microspheres, and achieve the goal of not being prone to sulfonic acid The effect of base content and large particle size

Active Publication Date: 2021-02-05
FUJIAN AGRI & FORESTRY UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a preparation method of polystyrene resin with high sulfonic acid group content on the surface, which solves the problem of the existing large-diameter sulfonated polystyrene resin microspheres in the polymerization process. During the process, due to the steric hindrance effect, the surface sulfonic acid group content is low and the distribution is uneven, the sulfonation polymerization process is dangerous, difficult to control, the strength of the resin microspheres is low, and the cost is high.

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  • Preparation method of highly sulfonated polystyrene resin

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preparation example Construction

[0020] The invention discloses a preparation method of highly sulfonated polystyrene resin, the method comprising the following steps:

[0021] Step 1. Pretreatment of unmodified polystyrene resin: Weigh a certain amount of polystyrene resin microspheres, add dichloromethane to swell for 5-15 hours, and then use tetrahydrofuran, ultrapure water, absolute ethanol, and anhydrous methanol Wash and filter each for 2-3 times, and finally vacuum-dry at 20-30°C to constant weight;

[0022] Step 2. Chloroacetylation of polystyrene resin microspheres: Weigh the polystyrene resin microspheres treated in step 1, add dichloromethane to the high-pressure reaction bottle to swell for 5-10 hours, and then add aluminum chloride to the reaction system React with chloroacetyl chloride at 25-50°C under high pressure for 1-5h, and finally filter off the reaction reagent, wash and filter with tetrahydrofuran, water, 3% mass fraction of dilute hydrochloric acid, absolute ethanol, and methanol for 2...

Embodiment 1

[0028] Example 1: Weigh 0.5g of polystyrene resin microspheres, add dichloromethane to swell for 5 hours, wash and filter with tetrahydrofuran, ultrapure water, absolute ethanol, and anhydrous methanol three times in a sand core funnel, and finally 20°C Dry in vacuo to constant weight.

[0029] Acylation of polystyrene resin microspheres: Weigh 0.3 g of pretreated polystyrene resin white balls, put them into a high-pressure reaction bottle and swell with 20 ml of dichloromethane for 5 h, add catalyst aluminum chloride 0.28 g, acetylation reagent ethyl chloride 100 μl of acid chloride was reacted in a water-bath shaker in a high-pressure reaction flask at 50°C for 5 hours. After cooling to room temperature, wash and filter twice with tetrahydrofuran, 3% dilute hydrochloric acid, ultrapure water, absolute ethanol, and methanol successively, and finally vacuum-dry at 30°C to constant weight to obtain chloroacetylated polystyrene resin microspheres.

[0030] Sulfonation modificatio...

Embodiment 2

[0031] Example 2: Weigh 0.5g of polystyrene resin microspheres, add dichloromethane to swell for 10 hours, wash and filter with tetrahydrofuran, ultrapure water, absolute ethanol, and anhydrous methanol three times in a sand core funnel, and finally 30°C Dry in vacuo to constant weight.

[0032] Acylation of polystyrene resin microspheres: Weigh 0.3 g of pretreated polystyrene resin white balls, put them into a high-pressure reaction bottle and swell with 20 ml of dichloromethane for 10 h, add catalyst aluminum chloride 0.59 g, acetylation reagent ethyl chloride 300 μl of acid chloride was reacted in a water-bath shaker in a high-pressure reaction bottle at 50°C for 5 hours. After cooling to room temperature, wash and filter twice with tetrahydrofuran, 3% dilute hydrochloric acid, ultrapure water, absolute ethanol, and methanol successively, and finally vacuum-dry at 30°C to constant weight to obtain chloroacetylated polystyrene resin microspheres.

[0033] Anionic modificati...

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Abstract

The invention provides a preparation method of highly sulfonated polystyrene resin. In the preparation method, adopted unmodified resin is large-particle polystyrene resin microspheres, and ananionicmonomer for modification adopts sodium p-styrenesulfonate. The preparation methodcomprises the following steps: swelling polystyrene resin microspheres by using dichloromethane, sequentially conducting washing and filtering by using tetrahydrofuran, ultrapure water, absolute ethyl alcohol and methanol for multiple times, and finally performing vacuum drying; then grafting an acylation reagent chloroacetyl chloride on the surfaces of the pretreated microspheres by utilizing a Friedel-Crafts acylation reaction to obtain an acylated polystyrene resin macromolecular initiator; and finally, initiating monomer sodium p-styrenesulfonate to polymerize on the surface of the polystyrene resin by utilizing an atom transfer radical polymerization method, taking cuprous bromide as a catalyst and takingpentamethyldiethylenetriamine as a ligand. The preparation method solves the problems that the amount of sulfonic acid groups is small, the reaction process is not easy to control, the strength of the resin microspheres is low and the cost is high due to the steric hindrance effect when the surfaces of the existing large-particle-size polystyrene resin microspheres are sulfonated.

Description

【Technical field】 [0001] The invention relates to a functional modification of polymers, in particular to a method for sulfonation modification of polystyrene resin microspheres. 【Background technique】 [0002] Polystyrene resin microspheres refer to rigid beads prepared with styrene as a monomer and divinylbenzene as a crosslinking agent, with diameters ranging from tens of nanometers to hundreds of microns. The different sizes determine the different physical properties of the microspheres. Nanoscale polystyrene resin microspheres are usually used as catalyst supports because of their relatively small surface energy. Micron-sized polystyrene resin microspheres have relatively large surface energy, and using them as catalyst supports cannot effectively reduce the reaction activation energy, but using them as adsorbents has a better effect. Compared with pure solid resin microspheres, resin microspheres with porous / vacuum structure have higher specific surface area and ads...

Claims

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Application Information

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IPC IPC(8): C08F8/18C08F8/36C08F112/08
CPCC08F8/36C08F8/18C08F112/08
Inventor 苗庆显孟令超蔡玉群张琛张凤山黄六莲
Owner FUJIAN AGRI & FORESTRY UNIV
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